Poly[μ-aqua-aqua­(μ-benzene-1,2,4,5-tetra­carboxyl­ato)gadolinate(III)potassium(I)]

Gong, X.Y.; Zhang, L.

doi:10.1107/S1600536811016254

metal-organic compounds

CRYSTALLOGRAPHIC
COMMUNICATIONS

ISSN: 2056-9890

Volume 67| Part 6| June 2011| Page m736

doi:10.1107/S1600536811016254

Open

access

Poly[μ-aqua-aqua(μ-benzene-1,2,4,5-tetracarboxylato)gadolinate(III)potassium(I)]

Xue Yun Gong ^a ^* and Lei Zhang ^a

^aDepartment of Physics and Chemistry, Henan Polytechnic University, Jiaozuo, Henan 454000, People's Republic of China
^*Correspondence e-mail: gxy@hpu.edu.cn

(Received 11 April 2011; accepted 29 April 2011; online 11 May 2011)

In the title compound, [KGd(C₁₀H₂O₈)(H₂O)₂]_n, the Gd³⁺ ion is nine-coordinated by eight O atoms from five individual benzene-1,2,4,5-tetracarboxylate (btec) ligands and one water molecule, and the K⁺ ion is eight-coordinated by six O atoms from five individual btec ligands and two water molecules. In the crystal, the btec half-molecules are completed by crystallographic inversion symmetry. GdO₉ and KO₈ polyhedra are connected, forming layers in the ab plane, which are further interconnected by μ₈- or μ₁₂-bridging btec ligands, forming a three-dimensional structure.

Related literature

For structures based on H₄btec ligand, see: Huang et al. (2009 ); Lu et al. (2005 ); Wu et al. (2001 ); Zhang et al. (2005 ). For the isotypic neodymium(III) compound, see: Dai et al. (2008 ).

Experimental

Crystal data

[KGd(C₁₀H₂O₈)(H₂O)₂]
M_r = 482.50
Monoclinic, P 2₁ /c
a = 8.9003 (1) Å
b = 7.7816 (1) Å
c = 17.5150 (3) Å
β = 91.857 (1)°
V = 1212.43 (3) Å³
Z = 4
Mo Kα radiation
μ = 5.87 mm⁻¹
T = 296 K
0.20 × 0.10 × 0.10 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.386, T_max = 0.591
14043 measured reflections
3002 independent reflections
2588 reflections with I > 2σ(I)
R_int = 0.037

Refinement

R[F² > 2σ(F²)] = 0.024
wR(F²) = 0.051
S = 1.04
3002 reflections
199 parameters
H-atom parameters constrained
Δρ_max = 0.91 e Å⁻³
Δρ_min = −1.29 e Å⁻³

Table 1
Selected bond lengths (Å)

Gd1—O6ⁱ	2.337 (3)
Gd1—O7ⁱⁱ	2.376 (2)
Gd1—O8	2.433 (2)
Gd1—O3	2.441 (2)
Gd1—O1	2.447 (3)
Gd1—O5ⁱⁱⁱ	2.451 (2)
Gd1—O4ⁱⁱⁱ	2.503 (2)
Gd1—O9	2.520 (3)
Gd1—O2	2.604 (2)
K1—O2	2.714 (3)
K1—O6	2.783 (3)
K1—O8	2.795 (3)
K1—O10	2.842 (3)
K1—O1^iv	2.860 (3)
K1—O4^iv	2.875 (3)
K1—O7ⁱ	2.891 (3)
K1—O9^v	2.893 (3)
Symmetry codes: (i) $[-x, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (ii) x, y-1, z; (iii) $[-x+1, y-{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (iv) $[-x+1, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ ; (v) $[-x, y+{\script{1\over 2}}, -z+{\script{3\over 2}}]$ .

Data collection: APEX2 (Bruker, 2008 ); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811016254/si2351sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536811016254/si2351Isup2.hkl

checkCIF report

Comment top

The btec ligand is a remarkably versatile building block for the construction of supramolecular architectures due to its four rigid carboxyl groups and various coordination modes in the self-assembly reaction (Huang et al., 2009; Lu et al., 2005; Wu et al., 2001; Zhang et al., 2005). Furthermore, they can provide directional conformation of network structures via noncovalent contacts like hydrogen bonding and aromatic stacking. In this paper, we report the preparation and crystal structure of a new potassium(I)-gadolinium(III) complex, [KGd(btec)(H₂O)₂]_n, where btec = benzene-1,2,4,5-tetracarboxylate. The crystal structures of a Ndⁱⁱⁱanalogue has been reported recently (Dai et al., 2008).

As shown in Fig. 1, the asymmetric building unit of title compound comprises one Gd^III atom, one K^I atom, two coordinated water molecules and two btec ligands. The two crystallographic distinct btec ligands occupy inversion symmetry in the structure. One of them acts as a µ₁₂-bridge linking six Gd^III and six K^I atoms, while the other one acts as a µ₈-bridge linking four Gd^III and four K^I atoms. Considering the linking environment of the gadolinium(III) and potassium(I) atoms, Gd^III is nine-coordinated by eight O atoms from five individual btec ligands and one water molecule, while the K^I atom is eight-coordinated by six O atoms from five individual btec ligands and two water molecules, as listed in Tab. 1. As shown in Fig. 2, when C and H atoms are omitted, a two-dimensional Gd—K—O framework is emerged in the ab plane. Furthermore, these two-dimensional layers are integrated by C atoms of btec ligands into a three-dimensional framework.

Related literature top

For structures based on H₄btec ligand, see: Huang et al. (2009); Lu et al. (2005); Wu et al. (2001); Zhang et al. (2005). For the isotypic neodymium(III) compound, see: Dai et al. (2008).

Experimental top

A mixture of 1,2,4,5-benzenetetracarboxylic (0.05 g), Gd₂O₃ (0.05 g), KOH(0.05 g) and H₂O (15 ml) was heated at 448 K for 7 d in a sealed 25 ml Teflon-lined stainless steel vessel under autogenous pressure. After cooling to room temperature at a rate of 5 C h^-1, colorless prismatic crystals were obtained in low yield.

Computing details top

Data collection: APEX2 (Bruker, 2008); cell refinement: SAINT (Bruker, 2008); data reduction: SAINT (Bruker, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

Fig. 1. The Gd^III and K^I coordination environment of the title compound indicating the inversion symmetry of the btec ligands by symmetry codes vii and viii. Displacement ellipsoids are drawn at the 50% probability level for non-H atoms. [Symmetry codes: (i) -x, y - 1/2, -z + 3/2; (ii) x, y - 1, z; (iii) -x + 1, y - 1/2, -z + 3/2; (iv) -x + 1, y + 1/2, -z + 3/2; (v) -x, y + 1/2, -z + 3/2; (vii) -x + 1, -y + 1, -z + 2; (viii) -x, -y + 2, -z + 1].

Fig. 2. View of the three-dimensional network for the title compound.

Poly[µ-aqua-aqua(µ-benzene-1,2,4,5- tetracarboxylato)gadolinate(III)potassium(I)] top

Crystal data top

[KGd(C₁₀H₂O₈)(H₂O)₂]	F(000) = 916
M_r = 482.50	D_x = 2.643 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2537 reflections
a = 8.9003 (1) Å	θ = 2.3–25.1°
b = 7.7816 (1) Å	µ = 5.87 mm⁻¹
c = 17.5150 (3) Å	T = 296 K
β = 91.857 (1)°	Prism, colourless
V = 1212.43 (3) Å³	0.20 × 0.10 × 0.10 mm
Z = 4

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	3002 independent reflections
Radiation source: fine-focus sealed tube	2588 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.037
Detector resolution: 83.33 pixels mm^-1	θ_max = 28.3°, θ_min = 2.3°
ω scans	h = −11→11
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −10→9
T_min = 0.386, T_max = 0.591	l = −23→23
14043 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.051	H-atom parameters constrained
S = 1.04	w = 1/[σ²(F_o²) + (0.0208P)² + 1.8584P] where P = (F_o² + 2F_c²)/3
3002 reflections	(Δ/σ)_max = 0.002
199 parameters	Δρ_max = 0.91 e Å⁻³
0 restraints	Δρ_min = −1.29 e Å⁻³

Crystal data top

[KGd(C₁₀H₂O₈)(H₂O)₂]	V = 1212.43 (3) Å³
M_r = 482.50	Z = 4
Monoclinic, P2₁/c	Mo Kα radiation
a = 8.9003 (1) Å	µ = 5.87 mm⁻¹
b = 7.7816 (1) Å	T = 296 K
c = 17.5150 (3) Å	0.20 × 0.10 × 0.10 mm
β = 91.857 (1)°

Data collection top

Bruker SMART APEXII CCD area-detector diffractometer	3002 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	2588 reflections with I > 2σ(I)
T_min = 0.386, T_max = 0.591	R_int = 0.037
14043 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.024	0 restraints
wR(F²) = 0.051	H-atom parameters constrained
S = 1.04	Δρ_max = 0.91 e Å⁻³
3002 reflections	Δρ_min = −1.29 e Å⁻³
199 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq
Gd1	0.21753 (2)	0.47536 (2)	0.699264 (9)	0.00997 (6)
K1	0.22962 (11)	0.97212 (11)	0.78942 (5)	0.02529 (19)
O1	0.4699 (3)	0.5723 (3)	0.66830 (15)	0.0226 (6)
H1A	0.5081	0.6065	0.7107	0.027*
H1B	0.4533	0.6604	0.6406	0.027*
C1	0.3791 (4)	0.5106 (4)	0.8437 (2)	0.0147 (7)
O2	0.3319 (3)	0.6478 (3)	0.81457 (14)	0.0183 (6)
C2	0.4485 (4)	0.5076 (4)	0.92329 (19)	0.0128 (7)
O3	0.3601 (3)	0.3676 (3)	0.81063 (14)	0.0210 (6)
C3	0.3828 (4)	0.3974 (4)	0.97488 (18)	0.0142 (7)
H3	0.3041	0.3270	0.9581	0.017*
O4	0.6594 (3)	0.6935 (3)	0.82750 (13)	0.0180 (6)
C4	0.5683 (4)	0.6106 (4)	0.94877 (18)	0.0128 (7)
O5	0.7106 (3)	0.8636 (3)	0.92519 (13)	0.0173 (6)
C5	0.6512 (4)	0.7290 (4)	0.89702 (19)	0.0139 (7)
O6	−0.0404 (3)	1.0020 (3)	0.70586 (14)	0.0163 (5)
C6	0.0794 (4)	0.7479 (4)	0.61673 (19)	0.0129 (7)
O7	0.0284 (3)	1.2656 (3)	0.67405 (14)	0.0168 (5)
C7	0.0324 (4)	0.8804 (4)	0.55820 (18)	0.0105 (7)
O8	0.1973 (3)	0.7726 (3)	0.65718 (14)	0.0189 (6)
C8	0.0245 (4)	0.8287 (4)	0.48207 (18)	0.0118 (7)
H8	0.0403	0.7138	0.4700	0.014*
O9	0.0079 (3)	0.6102 (3)	0.61982 (15)	0.0236 (6)
C9	0.0067 (4)	1.0533 (4)	0.57629 (19)	0.0121 (7)
C10	−0.0015 (4)	1.1124 (4)	0.65777 (18)	0.0107 (7)
H10A	0.3331	1.0155	0.9851	0.013*
H10B	0.4337	0.9339	0.9384	0.013*
O10	0.3392 (4)	0.9561 (4)	0.94345 (18)	0.0398 (8)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Gd1	0.01314 (10)	0.00955 (8)	0.00718 (8)	0.00160 (7)	−0.00007 (6)	−0.00017 (6)
K1	0.0245 (5)	0.0240 (4)	0.0270 (5)	−0.0026 (4)	−0.0061 (4)	0.0027 (3)
O1	0.0190 (15)	0.0213 (13)	0.0278 (15)	−0.0025 (11)	0.0022 (12)	−0.0034 (11)
C1	0.0161 (19)	0.0175 (17)	0.0104 (16)	0.0008 (14)	0.0006 (14)	0.0011 (13)
O2	0.0226 (15)	0.0168 (13)	0.0153 (13)	−0.0012 (11)	−0.0046 (11)	0.0045 (10)
C2	0.0161 (19)	0.0125 (16)	0.0096 (16)	0.0008 (13)	−0.0010 (13)	0.0008 (12)
O3	0.0335 (17)	0.0156 (12)	0.0133 (13)	0.0060 (11)	−0.0071 (12)	−0.0033 (10)
C3	0.0158 (19)	0.0157 (17)	0.0111 (16)	−0.0033 (14)	−0.0003 (14)	0.0000 (13)
O4	0.0225 (15)	0.0206 (13)	0.0109 (12)	−0.0066 (11)	0.0026 (11)	0.0019 (10)
C4	0.0151 (19)	0.0140 (17)	0.0092 (16)	0.0013 (14)	0.0001 (14)	0.0018 (13)
O5	0.0225 (15)	0.0175 (12)	0.0121 (12)	−0.0048 (11)	0.0011 (11)	0.0015 (10)
C5	0.0122 (18)	0.0161 (17)	0.0134 (17)	0.0005 (14)	0.0003 (14)	0.0050 (13)
O6	0.0220 (14)	0.0159 (13)	0.0111 (12)	0.0023 (10)	0.0044 (10)	0.0046 (9)
C6	0.020 (2)	0.0116 (16)	0.0075 (15)	0.0030 (14)	0.0051 (14)	−0.0011 (12)
O7	0.0199 (15)	0.0144 (12)	0.0161 (13)	−0.0036 (10)	0.0023 (11)	−0.0040 (10)
C7	0.0137 (18)	0.0095 (15)	0.0083 (15)	−0.0020 (13)	0.0009 (13)	0.0015 (12)
O8	0.0193 (15)	0.0172 (13)	0.0199 (14)	0.0003 (11)	−0.0055 (11)	0.0045 (10)
C8	0.0151 (19)	0.0109 (16)	0.0096 (16)	0.0013 (13)	0.0026 (13)	−0.0005 (12)
O9	0.0280 (17)	0.0165 (13)	0.0255 (15)	−0.0050 (11)	−0.0090 (12)	0.0082 (11)
C9	0.0133 (18)	0.0117 (16)	0.0112 (16)	−0.0010 (13)	−0.0001 (13)	0.0004 (12)
C10	0.0106 (18)	0.0124 (16)	0.0090 (15)	0.0034 (13)	0.0008 (13)	0.0010 (12)
O10	0.045 (2)	0.046 (2)	0.0290 (17)	−0.0029 (16)	0.0128 (15)	−0.0107 (14)

Geometric parameters (Å, º) top

Gd1—O6ⁱ	2.337 (3)	C2—C4	1.396 (5)
Gd1—O7ⁱⁱ	2.376 (2)	O3—K1ⁱⁱ	3.306 (3)
Gd1—O8	2.433 (2)	C3—C4^vii	1.394 (4)
Gd1—O3	2.441 (2)	C3—H3	0.9300
Gd1—O1	2.447 (3)	O4—C5	1.253 (4)
Gd1—O5ⁱⁱⁱ	2.451 (2)	O4—Gd1^iv	2.503 (2)
Gd1—O4ⁱⁱⁱ	2.503 (2)	O4—K1ⁱⁱⁱ	2.875 (3)
Gd1—O9	2.520 (3)	C4—C3^vii	1.394 (4)
Gd1—O2	2.604 (2)	C4—C5	1.502 (5)
Gd1—C6	2.825 (3)	O5—C5	1.266 (4)
Gd1—C5ⁱⁱⁱ	2.831 (3)	O5—Gd1^iv	2.451 (2)
Gd1—C1	2.882 (3)	C5—Gd1^iv	2.831 (3)
K1—O2	2.714 (3)	O6—C10	1.259 (4)
K1—O6	2.783 (3)	O6—Gd1^v	2.337 (3)
K1—O8	2.795 (3)	C6—O9	1.249 (4)
K1—O10	2.842 (3)	C6—O8	1.261 (4)
K1—O1^iv	2.860 (3)	C6—C7	1.504 (4)
K1—O4^iv	2.875 (3)	O7—C10	1.253 (4)
K1—O7ⁱ	2.891 (3)	O7—Gd1^vi	2.376 (2)
K1—O9^v	2.893 (3)	O7—K1^v	2.891 (3)
K1—C10	3.230 (3)	C7—C8	1.392 (4)
K1—O3^vi	3.306 (3)	C7—C9	1.402 (5)
K1—Gd1^v	3.9912 (10)	C8—C9^viii	1.396 (4)
O1—K1ⁱⁱⁱ	2.860 (3)	C8—H8	0.9300
O1—H1A	0.8501	O9—K1ⁱ	2.893 (3)
O1—H1B	0.8500	C9—C8^viii	1.396 (4)
C1—O2	1.250 (4)	C9—C10	1.503 (4)
C1—O3	1.263 (4)	O10—H10A	0.8671
C1—C2	1.506 (4)	O10—H10B	0.8656
C2—C3	1.388 (5)

O6ⁱ—Gd1—O7ⁱⁱ	72.72 (8)	O6—K1—O3^vi	105.99 (7)
O6ⁱ—Gd1—O8	94.93 (9)	O8—K1—O3^vi	129.52 (7)
O7ⁱⁱ—Gd1—O8	123.50 (8)	O10—K1—O3^vi	79.96 (8)
O6ⁱ—Gd1—O3	78.90 (9)	O1^iv—K1—O3^vi	52.77 (7)
O7ⁱⁱ—Gd1—O3	105.04 (9)	O4^iv—K1—O3^vi	52.76 (7)
O8—Gd1—O3	126.89 (8)	O7ⁱ—K1—O3^vi	140.46 (8)
O6ⁱ—Gd1—O1	140.86 (9)	O9^v—K1—O3^vi	81.54 (7)
O7ⁱⁱ—Gd1—O1	145.14 (9)	C10—K1—O3^vi	88.80 (7)
O8—Gd1—O1	72.49 (9)	O2—K1—Gd1^v	109.12 (6)
O3—Gd1—O1	79.97 (9)	O6—K1—Gd1^v	34.92 (5)
O6ⁱ—Gd1—O5ⁱⁱⁱ	149.95 (9)	O8—K1—Gd1^v	88.21 (6)
O7ⁱⁱ—Gd1—O5ⁱⁱⁱ	78.16 (8)	O10—K1—Gd1^v	105.38 (8)
O8—Gd1—O5ⁱⁱⁱ	94.98 (8)	O1^iv—K1—Gd1^v	155.64 (6)
O3—Gd1—O5ⁱⁱⁱ	116.41 (8)	O4^iv—K1—Gd1^v	113.43 (6)
O1—Gd1—O5ⁱⁱⁱ	69.16 (9)	O7ⁱ—K1—Gd1^v	36.12 (5)
O6ⁱ—Gd1—O4ⁱⁱⁱ	121.37 (8)	O9^v—K1—Gd1^v	38.99 (5)
O7ⁱⁱ—Gd1—O4ⁱⁱⁱ	71.02 (8)	C10—K1—Gd1^v	54.57 (6)
O8—Gd1—O4ⁱⁱⁱ	143.63 (9)	O3^vi—K1—Gd1^v	109.62 (5)
O3—Gd1—O4ⁱⁱⁱ	68.24 (8)	O2—K1—Gd1	37.34 (5)
O1—Gd1—O4ⁱⁱⁱ	79.53 (9)	O6—K1—Gd1	82.38 (5)
O5ⁱⁱⁱ—Gd1—O4ⁱⁱⁱ	52.70 (8)	O8—K1—Gd1	34.09 (5)
O6ⁱ—Gd1—O9	81.44 (9)	O10—K1—Gd1	108.80 (7)
O7ⁱⁱ—Gd1—O9	71.09 (8)	O1^iv—K1—Gd1	111.26 (6)
O8—Gd1—O9	52.45 (8)	O4^iv—K1—Gd1	106.89 (5)
O3—Gd1—O9	160.19 (9)	O7ⁱ—K1—Gd1	63.78 (5)
O1—Gd1—O9	114.70 (9)	O9^v—K1—Gd1	122.78 (6)
O5ⁱⁱⁱ—Gd1—O9	82.34 (9)	C10—K1—Gd1	92.00 (6)
O4ⁱⁱⁱ—Gd1—O9	125.60 (8)	O3^vi—K1—Gd1	155.35 (6)
O6ⁱ—Gd1—O2	70.03 (8)	Gd1^v—K1—Gd1	90.638 (18)
O7ⁱⁱ—Gd1—O2	139.01 (8)	Gd1—O1—K1ⁱⁱⁱ	135.72 (11)
O8—Gd1—O2	76.60 (8)	Gd1—O1—H1A	104.3
O3—Gd1—O2	51.49 (8)	K1ⁱⁱⁱ—O1—H1A	61.0
O1—Gd1—O2	71.01 (9)	Gd1—O1—H1B	103.4
O5ⁱⁱⁱ—Gd1—O2	139.97 (9)	K1ⁱⁱⁱ—O1—H1B	120.7
O4ⁱⁱⁱ—Gd1—O2	115.76 (8)	H1A—O1—H1B	107.7
O9—Gd1—O2	118.52 (8)	O2—C1—O3	121.8 (3)
O6ⁱ—Gd1—C6	90.28 (9)	O2—C1—C2	120.9 (3)
O7ⁱⁱ—Gd1—C6	97.28 (10)	O3—C1—C2	117.1 (3)
O8—Gd1—C6	26.43 (9)	O2—C1—Gd1	64.62 (18)
O3—Gd1—C6	150.81 (9)	O3—C1—Gd1	57.19 (17)
O1—Gd1—C6	92.43 (10)	C2—C1—Gd1	171.3 (2)
O5ⁱⁱⁱ—Gd1—C6	86.17 (9)	C1—O2—Gd1	89.7 (2)
O4ⁱⁱⁱ—Gd1—C6	138.40 (8)	C1—O2—K1	165.2 (2)
O9—Gd1—C6	26.23 (9)	Gd1—O2—K1	103.46 (8)
O2—Gd1—C6	99.35 (8)	C3—C2—C4	118.7 (3)
O6ⁱ—Gd1—C5ⁱⁱⁱ	141.71 (9)	C3—C2—C1	116.3 (3)
O7ⁱⁱ—Gd1—C5ⁱⁱⁱ	74.19 (9)	C4—C2—C1	125.0 (3)
O8—Gd1—C5ⁱⁱⁱ	119.44 (10)	C1—O3—Gd1	97.0 (2)
O3—Gd1—C5ⁱⁱⁱ	91.69 (9)	C1—O3—K1ⁱⁱ	155.9 (2)
O1—Gd1—C5ⁱⁱⁱ	71.17 (9)	Gd1—O3—K1ⁱⁱ	93.34 (8)
O5ⁱⁱⁱ—Gd1—C5ⁱⁱⁱ	26.51 (9)	C2—C3—C4^vii	121.8 (3)
O4ⁱⁱⁱ—Gd1—C5ⁱⁱⁱ	26.26 (9)	C2—C3—H3	119.1
O9—Gd1—C5ⁱⁱⁱ	105.40 (9)	C4^vii—C3—H3	119.1
O2—Gd1—C5ⁱⁱⁱ	130.73 (9)	C5—O4—Gd1^iv	91.6 (2)
C6—Gd1—C5ⁱⁱⁱ	112.63 (10)	C5—O4—K1ⁱⁱⁱ	148.9 (2)
O6ⁱ—Gd1—C1	72.32 (10)	Gd1^iv—O4—K1ⁱⁱⁱ	103.25 (9)
O7ⁱⁱ—Gd1—C1	123.98 (9)	C3^vii—C4—C2	119.5 (3)
O8—Gd1—C1	101.85 (9)	C3^vii—C4—C5	117.5 (3)
O3—Gd1—C1	25.79 (9)	C2—C4—C5	123.0 (3)
O1—Gd1—C1	74.32 (10)	C5—O5—Gd1^iv	93.7 (2)
O5ⁱⁱⁱ—Gd1—C1	132.62 (10)	O4—C5—O5	121.6 (3)
O4ⁱⁱⁱ—Gd1—C1	92.23 (9)	O4—C5—C4	119.8 (3)
O9—Gd1—C1	141.67 (9)	O5—C5—C4	118.6 (3)
O2—Gd1—C1	25.71 (8)	O4—C5—Gd1^iv	62.10 (18)
C6—Gd1—C1	125.03 (10)	O5—C5—Gd1^iv	59.77 (18)
C5ⁱⁱⁱ—Gd1—C1	112.55 (10)	C4—C5—Gd1^iv	174.2 (2)
O2—K1—O6	116.27 (8)	C10—O6—Gd1^v	138.0 (2)
O2—K1—O8	69.09 (7)	C10—O6—K1	99.1 (2)
O6—K1—O8	63.05 (8)	Gd1^v—O6—K1	102.10 (9)
O2—K1—O10	72.67 (9)	O9—C6—O8	121.5 (3)
O6—K1—O10	140.08 (10)	O9—C6—C7	119.1 (3)
O8—K1—O10	141.74 (9)	O8—C6—C7	119.1 (3)
O2—K1—O1^iv	84.58 (8)	O9—C6—Gd1	63.11 (18)
O6—K1—O1^iv	153.86 (8)	O8—C6—Gd1	59.14 (17)
O8—K1—O1^iv	115.86 (9)	C7—C6—Gd1	166.0 (2)
O10—K1—O1^iv	58.46 (9)	C10—O7—Gd1^vi	147.2 (2)
O2—K1—O4^iv	123.48 (8)	C10—O7—K1^v	114.5 (2)
O6—K1—O4^iv	83.45 (7)	Gd1^vi—O7—K1^v	98.05 (8)
O8—K1—O4^iv	76.77 (7)	C8—C7—C9	119.4 (3)
O10—K1—O4^iv	125.96 (9)	C8—C7—C6	117.3 (3)
O1^iv—K1—O4^iv	71.42 (8)	C9—C7—C6	123.2 (3)
O2—K1—O7ⁱ	73.25 (8)	C6—O8—Gd1	94.4 (2)
O6—K1—O7ⁱ	58.96 (7)	C6—O8—K1	127.7 (2)
O8—K1—O7ⁱ	79.25 (8)	Gd1—O8—K1	105.81 (9)
O10—K1—O7ⁱ	90.92 (9)	C7—C8—C9^viii	120.9 (3)
O1^iv—K1—O7ⁱ	146.80 (8)	C7—C8—H8	119.5
O4^iv—K1—O7ⁱ	141.64 (7)	C9^viii—C8—H8	119.5
O2—K1—O9^v	120.23 (8)	C6—O9—Gd1	90.7 (2)
O6—K1—O9^v	67.91 (7)	C6—O9—K1ⁱ	136.5 (2)
O8—K1—O9^v	127.17 (8)	Gd1—O9—K1ⁱ	94.77 (8)
O10—K1—O9^v	74.28 (9)	C8^viii—C9—C7	119.7 (3)
O1^iv—K1—O9^v	116.76 (8)	C8^viii—C9—C10	118.6 (3)
O4^iv—K1—O9^v	116.29 (8)	C7—C9—C10	121.4 (3)
O7ⁱ—K1—O9^v	59.01 (7)	O7—C10—O6	123.9 (3)
O2—K1—C10	129.24 (8)	O7—C10—C9	119.4 (3)
O6—K1—C10	22.64 (8)	O6—C10—C9	116.7 (3)
O8—K1—C10	63.26 (8)	O7—C10—K1	91.9 (2)
O10—K1—C10	152.09 (10)	O6—C10—K1	58.30 (18)
O1^iv—K1—C10	131.40 (9)	C9—C10—K1	121.7 (2)
O4^iv—K1—C10	60.96 (8)	K1—O10—H10A	138.3
O7ⁱ—K1—C10	81.59 (8)	K1—O10—H10B	102.5
O9^v—K1—C10	78.87 (8)	H10A—O10—H10B	106.3
O2—K1—O3^vi	137.10 (8)

Symmetry codes: (i) −x, y−1/2, −z+3/2; (ii) x, y−1, z; (iii) −x+1, y−1/2, −z+3/2; (iv) −x+1, y+1/2, −z+3/2; (v) −x, y+1/2, −z+3/2; (vi) x, y+1, z; (vii) −x+1, −y+1, −z+2; (viii) −x, −y+2, −z+1.

Experimental details

Crystal data
Chemical formula	[KGd(C₁₀H₂O₈)(H₂O)₂]
M_r	482.50
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	296
a, b, c (Å)	8.9003 (1), 7.7816 (1), 17.5150 (3)
β (°)	91.857 (1)
V (Å³)	1212.43 (3)
Z	4
Radiation type	Mo Kα
µ (mm⁻¹)	5.87
Crystal size (mm)	0.20 × 0.10 × 0.10

Data collection
Diffractometer	Bruker SMART APEXII CCD area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.386, 0.591
No. of measured, independent and observed [I > 2σ(I)] reflections	14043, 3002, 2588
R_int	0.037
(sin θ/λ)_max (Å⁻¹)	0.666

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.024, 0.051, 1.04
No. of reflections	3002
No. of parameters	199
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.91, −1.29

Computer programs: APEX2 (Bruker, 2008), SAINT (Bruker, 2008), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

Selected bond lengths (Å) top

Gd1—O6ⁱ	2.337 (3)	K1—O2	2.714 (3)
Gd1—O7ⁱⁱ	2.376 (2)	K1—O6	2.783 (3)
Gd1—O8	2.433 (2)	K1—O8	2.795 (3)
Gd1—O3	2.441 (2)	K1—O10	2.842 (3)
Gd1—O1	2.447 (3)	K1—O1^iv	2.860 (3)
Gd1—O5ⁱⁱⁱ	2.451 (2)	K1—O4^iv	2.875 (3)
Gd1—O4ⁱⁱⁱ	2.503 (2)	K1—O7ⁱ	2.891 (3)
Gd1—O9	2.520 (3)	K1—O9^v	2.893 (3)
Gd1—O2	2.604 (2)

Symmetry codes: (i) −x, y−1/2, −z+3/2; (ii) x, y−1, z; (iii) −x+1, y−1/2, −z+3/2; (iv) −x+1, y+1/2, −z+3/2; (v) −x, y+1/2, −z+3/2.

References

Bruker (2008). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
Dai, Y. M., Tang, E., Wang, X. Q., Huang, J. F., Wang, L. H. & Huang, X. D. (2008). Chin. J. Struct. Chem. 27, 1031–1034. CAS Google Scholar
Huang, R. Y., Xu, H. M., Zhu, K., Liu, G. X. & Ren, X. M. (2009). Chin. J. Struct. Chem. 28, 1661–1665. CAS Google Scholar
Lu, K. L., Chen, Y. F., Liu, Y. H., Cheng, Y. W., Liao, R. T. & Wen, Y. S. (2005). Cryst. Growth Des. 5, 403–407. CrossRef CAS Google Scholar
Sheldrick, G. M. (1996). SADABS. University of Göttingen, Germany. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Wu, C. D., Lu, C. Z., Wu, D. M., Zhuang, H. H. & Huang, J. S. (2001). Inorg. Chem. Commun. 4, 561–564. CrossRef CAS Google Scholar
Zhang, L. J., Yu, J. H., Xu, J. Q., Lu, J., Bie, H. Y. & Zhang, X. (2005). Inorg. Chem. Commun. 8, 638–642. CrossRef CAS Google Scholar

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.